# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
#===============================================================================
_audit_creation_date             2011-10-12

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Nicolas Mezailles'
_publ_contact_author_address     
;Laboratoire DCPH
Ecole Polytechnique
Route de Saclay
F91128 Palaiseau
France
;
_publ_contact_author_email       nicolas.mezailles@polytechnique.edu
_publ_contact_author_phone       330169334402
_publ_contact_author_fax         330169334440

_publ_contact_letter             
;
Please consider this CIF submission for publication as a new structure
paper in CHEMICAL COMMUNICATIONS. The figures, chemical
structure diagram (scheme), Transfert of Copyright Agreement form and
structure factors will be sent on receipt of your acknowledgement letter
;
#===============================================================================

# 2. PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic    ?

_journal_date_to_coeditor        ?
_journal_date_from_coeditor      ?
_journal_date_accepted           ?

_journal_date_printers_first     ?
_journal_date_printers_final     ?
_journal_date_proofs_out         ?
_journal_date_proofs_in          ?

_journal_coeditor_name           ?
_journal_coeditor_code           ?
_journal_coeditor_notes          
; ?
;

_journal_techeditor_code         ?
_journal_techeditor_notes        
; ?
;

_journal_coden_ASTM              ?
_journal_year                    ?
_journal_volume                  ?

_journal_issue                   ?
_journal_page_first              ?
_journal_page_last               ?

_journal_suppl_publ_number       ?
_journal_suppl_publ_pages        ?

#===============================================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;
Transmetalation of Nucleophilic Carbene Fragment:
from Early to Late Transition Metals
;
_publ_author_address             
;
a) Laboratoire Heteroelements et Coordination,
Ecole Polytechnique, CNRS
F-91128 Palaiseau Cedex
;

#===============================================================================
# 4. TEXT

_publ_section_abstract           
; ?
;

_publ_section_comment            
;
;
_publ_section_exptl_prep         
;All structures were solved using SIR97 (Altomare et al.) and refined with
SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990).
;

_publ_section_references         
;Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A.
(1993) J. Appl. Cryst. 26, 343-350.

Sheldrick, G.M. SHELXL97. Program for crystal structure
refinement. University of G\\"ottingen, Germany, 1997.

Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201.

Spek, A.L. (1990). Acta Cryst. A46, C-34.

Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7
;

_publ_section_figure_captions    
; ?
;

_publ_section_acknowledgements   
; ?
;
loop_
_publ_author_name
'N. Mezailles'
'M. Fustier'
'H. Heuclin'
'X. F. Le Goff'

#===============================================================================
# If more than one structure is reported, sections 5-10 should be filled in
# per structure. For each data set, replace the ? in the data_? line below
# by a unique identifier.

#===============================================================================

data_hh726
_database_code_depnum_ccdc_archive 'CCDC 848404'
#TrackingRef '2011_fustier_chemcommun.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H32 Cl2 O2 P2 S2 Zr, C4 H8 O'
_chemical_formula_sum            'C37 H40 Cl2 O3 P2 S2 Zr'
_chemical_formula_weight         820.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P3121 '
_symmetry_space_group_name_Hall  'P 31 2"'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
'y, x, -z'

_cell_length_a                   12.072(1)
_cell_length_b                   12.072(1)
_cell_length_c                   22.609(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2853.4(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    2264
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      30.034

_exptl_crystal_description       Block
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1266
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8688
_exptl_absorpt_correction_T_max  0.9020
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13053
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         27.47
_reflns_number_total             4300
_reflns_number_gt                4193
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_reduction        'DENZO & COLLECT'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.436 0.167 140 51 ' '
2 0.437 1.000 0.833 140 51 ' '
3 0.563 0.563 0.500 139 50 ' '
_platon_squeeze_details          
;
A highly disordered C4H8O molecule was accounted for using the
Platon SQUEEZE function
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+2.4598P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_number_reflns         4300
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0945
_refine_ls_wR_factor_gt          0.0939
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.10865(3) 0.0000 0.3333 0.02348(10) Uani 1 2 d S . .
P1 P 0.37390(7) 0.09189(7) 0.39071(3) 0.02566(15) Uani 1 1 d . . .
S1 S 0.24738(7) 0.13456(8) 0.42733(3) 0.03329(17) Uani 1 1 d . . .
Cl1 Cl -0.01636(8) -0.19833(8) 0.39144(4) 0.03882(18) Uani 1 1 d . . .
O1 O -0.0845(2) -0.0709(2) 0.28073(10) 0.0338(5) Uani 1 1 d . . .
C1 C 0.2897(3) 0.0000 0.3333 0.0265(8) Uani 1 2 d S . .
C2 C 0.5187(3) 0.2376(3) 0.36934(13) 0.0304(6) Uani 1 1 d . . .
C3 C 0.5139(4) 0.3470(4) 0.3570(2) 0.0509(9) Uani 1 1 d . . .
H3 H 0.4370 0.3486 0.3639 0.061 Uiso 1 1 calc R . .
C4 C 0.6201(5) 0.4549(4) 0.3348(2) 0.0649(12) Uani 1 1 d . . .
H4 H 0.6158 0.5298 0.3265 0.078 Uiso 1 1 calc R . .
C5 C 0.7324(4) 0.4535(4) 0.32457(18) 0.0531(10) Uani 1 1 d . . .
H5 H 0.8057 0.5275 0.3099 0.064 Uiso 1 1 calc R . .
C6 C 0.7368(4) 0.3449(4) 0.3358(2) 0.0584(11) Uani 1 1 d . . .
H6 H 0.8133 0.3431 0.3281 0.070 Uiso 1 1 calc R . .
C7 C 0.6311(3) 0.2367(4) 0.35838(19) 0.0485(9) Uani 1 1 d . . .
H7 H 0.6359 0.1620 0.3663 0.058 Uiso 1 1 calc R . .
C8 C 0.4271(3) 0.0175(3) 0.44467(13) 0.0297(6) Uani 1 1 d . . .
C9 C 0.5160(4) 0.0892(4) 0.48806(16) 0.0433(8) Uani 1 1 d . . .
H9 H 0.5486 0.1789 0.4904 0.052 Uiso 1 1 calc R . .
C10 C 0.5571(4) 0.0293(4) 0.52812(17) 0.0512(10) Uani 1 1 d . . .
H10 H 0.6197 0.0789 0.5570 0.061 Uiso 1 1 calc R . .
C11 C 0.5082(4) -0.0997(4) 0.52614(16) 0.0458(9) Uani 1 1 d . . .
H11 H 0.5367 -0.1398 0.5536 0.055 Uiso 1 1 calc R . .
C12 C 0.4178(4) -0.1718(4) 0.48446(17) 0.0484(9) Uani 1 1 d . . .
H12 H 0.3831 -0.2618 0.4837 0.058 Uiso 1 1 calc R . .
C13 C 0.3762(3) -0.1144(3) 0.44324(15) 0.0382(7) Uani 1 1 d . . .
H13 H 0.3138 -0.1649 0.4145 0.046 Uiso 1 1 calc R . .
C14 C -0.1820(4) -0.2049(4) 0.2689(3) 0.0724(15) Uani 1 1 d . . .
H14A H -0.1501 -0.2440 0.2400 0.087 Uiso 1 1 calc R . .
H14B H -0.2060 -0.2559 0.3058 0.087 Uiso 1 1 calc R . .
C15 C -0.2910(5) -0.1985(7) 0.2449(4) 0.103(2) Uani 1 1 d . . .
H15 H -0.3727 -0.2708 0.2374 0.123 Uiso 1 1 calc R . .
C16 C -0.2588(5) -0.0709(7) 0.2343(5) 0.145(4) Uani 1 1 d . . .
H16 H -0.3149 -0.0422 0.2211 0.174 Uiso 1 1 calc R . .
C17 C -0.1180(5) 0.0115(5) 0.2478(3) 0.0839(19) Uani 1 1 d . . .
H17A H -0.0676 0.0417 0.2109 0.101 Uiso 1 1 calc R . .
H17B H -0.1021 0.0866 0.2718 0.101 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.01884(13) 0.01989(17) 0.03207(18) 0.00189(14) 0.00095(7) 0.00994(9)
P1 0.0225(3) 0.0270(3) 0.0289(3) -0.0034(3) -0.0019(3) 0.0134(3)
S1 0.0297(4) 0.0382(4) 0.0364(4) -0.0088(3) -0.0012(3) 0.0203(3)
Cl1 0.0402(4) 0.0265(3) 0.0503(4) 0.0133(3) 0.0088(3) 0.0171(3)
O1 0.0222(10) 0.0298(10) 0.0475(12) 0.0019(8) -0.0057(9) 0.0116(9)
C1 0.0216(13) 0.030(2) 0.0304(19) -0.0026(15) -0.0013(8) 0.0152(10)
C2 0.0280(14) 0.0271(14) 0.0311(13) -0.0021(11) -0.0042(11) 0.0101(12)
C3 0.046(2) 0.0362(19) 0.069(2) 0.0073(17) 0.0114(18) 0.0188(16)
C4 0.067(3) 0.037(2) 0.083(3) 0.015(2) 0.018(3) 0.020(2)
C5 0.040(2) 0.042(2) 0.051(2) 0.0093(17) 0.0050(16) 0.0009(16)
C6 0.0305(18) 0.066(3) 0.068(3) 0.016(2) 0.0054(18) 0.0164(19)
C7 0.0312(16) 0.047(2) 0.066(2) 0.0135(18) 0.0021(16) 0.0184(15)
C8 0.0250(13) 0.0346(15) 0.0303(13) 0.0014(11) 0.0011(10) 0.0154(12)
C9 0.0420(19) 0.0413(18) 0.0403(17) -0.0017(14) -0.0116(14) 0.0160(15)
C10 0.041(2) 0.067(3) 0.0433(19) -0.0003(18) -0.0138(15) 0.026(2)
C11 0.0401(19) 0.068(3) 0.0388(17) 0.0157(17) 0.0046(14) 0.0341(19)
C12 0.054(2) 0.043(2) 0.051(2) 0.0104(17) 0.0014(17) 0.0263(18)
C13 0.0387(17) 0.0353(15) 0.0381(15) 0.0025(13) -0.0011(13) 0.0166(14)
C14 0.040(2) 0.047(2) 0.114(4) -0.005(3) -0.023(2) 0.0095(19)
C15 0.036(2) 0.078(4) 0.177(7) -0.041(4) -0.043(3) 0.016(3)
C16 0.041(3) 0.099(5) 0.251(10) 0.083(6) -0.055(4) 0.002(3)
C17 0.040(2) 0.071(3) 0.124(5) 0.043(3) -0.021(3) 0.016(2)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 C1 2.185(4) . ?
Zr1 O1 2.364(2) 4 ?
Zr1 O1 2.364(2) . ?
Zr1 Cl1 2.4744(8) . ?
Zr1 Cl1 2.4745(8) 4 ?
Zr1 S1 2.6905(8) 4 ?
Zr1 S1 2.6905(8) . ?
Zr1 P1 3.1007(8) . ?
Zr1 P1 3.1008(8) 4 ?
P1 C1 1.6790(13) . ?
P1 C8 1.812(3) . ?
P1 C2 1.819(3) . ?
P1 S1 2.0175(10) . ?
O1 C17 1.452(5) . ?
O1 C14 1.473(5) . ?
C1 P1 1.6791(13) 4 ?
C2 C3 1.379(5) . ?
C2 C7 1.385(5) . ?
C3 C4 1.387(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.363(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.391(4) . ?
C8 C13 1.392(4) . ?
C9 C10 1.396(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.363(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.374(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.395(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.461(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.407(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.511(6) . ?
C16 H16 0.9500 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Zr1 O1 143.64(6) . 4 ?
C1 Zr1 O1 143.64(6) . . ?
O1 Zr1 O1 72.72(11) 4 . ?
C1 Zr1 Cl1 97.24(2) . . ?
O1 Zr1 Cl1 83.92(5) 4 . ?
O1 Zr1 Cl1 84.43(6) . . ?
C1 Zr1 Cl1 97.25(2) . 4 ?
O1 Zr1 Cl1 84.43(6) 4 4 ?
O1 Zr1 Cl1 83.92(5) . 4 ?
Cl1 Zr1 Cl1 165.51(4) . 4 ?
C1 Zr1 S1 71.303(17) . 4 ?
O1 Zr1 S1 145.04(6) 4 4 ?
O1 Zr1 S1 72.35(6) . 4 ?
Cl1 Zr1 S1 91.24(3) . 4 ?
Cl1 Zr1 S1 93.39(3) 4 4 ?
C1 Zr1 S1 71.304(17) . . ?
O1 Zr1 S1 72.35(6) 4 . ?
O1 Zr1 S1 145.04(6) . . ?
Cl1 Zr1 S1 93.39(3) . . ?
Cl1 Zr1 S1 91.24(3) 4 . ?
S1 Zr1 S1 142.61(3) 4 . ?
C1 Zr1 P1 31.372(14) . . ?
O1 Zr1 P1 112.33(6) 4 . ?
O1 Zr1 P1 174.40(6) . . ?
Cl1 Zr1 P1 98.35(3) . . ?
Cl1 Zr1 P1 94.03(3) 4 . ?
S1 Zr1 P1 102.64(2) 4 . ?
S1 Zr1 P1 39.99(2) . . ?
C1 Zr1 P1 31.372(14) . 4 ?
O1 Zr1 P1 174.39(6) 4 4 ?
O1 Zr1 P1 112.33(6) . 4 ?
Cl1 Zr1 P1 94.02(2) . 4 ?
Cl1 Zr1 P1 98.35(3) 4 4 ?
S1 Zr1 P1 39.99(2) 4 4 ?
S1 Zr1 P1 102.64(2) . 4 ?
P1 Zr1 P1 62.74(3) . 4 ?
C1 P1 C8 116.12(13) . . ?
C1 P1 C2 113.91(11) . . ?
C8 P1 C2 104.52(14) . . ?
C1 P1 S1 101.54(13) . . ?
C8 P1 S1 110.58(10) . . ?
C2 P1 S1 110.26(11) . . ?
C1 P1 Zr1 42.66(13) . . ?
C8 P1 Zr1 131.52(10) . . ?
C2 P1 Zr1 123.78(10) . . ?
S1 P1 Zr1 58.99(3) . . ?
P1 S1 Zr1 81.02(3) . . ?
C17 O1 C14 108.4(3) . . ?
C17 O1 Zr1 124.9(2) . . ?
C14 O1 Zr1 126.2(2) . . ?
P1 C1 P1 148.1(3) 4 . ?
P1 C1 Zr1 105.97(13) 4 . ?
P1 C1 Zr1 105.97(13) . . ?
C3 C2 C7 118.8(3) . . ?
C3 C2 P1 120.0(3) . . ?
C7 C2 P1 120.8(3) . . ?
C2 C3 C4 120.7(4) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 119.4(4) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C7 120.9(4) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C2 C7 C6 120.2(4) . . ?
C2 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C9 C8 C13 119.4(3) . . ?
C9 C8 P1 121.4(3) . . ?
C13 C8 P1 119.3(2) . . ?
C8 C9 C10 119.9(4) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 120.5(4) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 119.9(3) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 120.9(4) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C8 C13 C12 119.3(3) . . ?
C8 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C15 C14 O1 104.8(4) . . ?
C15 C14 H14A 110.8 . . ?
O1 C14 H14A 110.8 . . ?
C15 C14 H14B 110.8 . . ?
O1 C14 H14B 110.8 . . ?
H14A C14 H14B 108.9 . . ?
C16 C15 C14 111.0(4) . . ?
C16 C15 H15 124.5 . . ?
C14 C15 H15 124.5 . . ?
C15 C16 C17 106.8(5) . . ?
C15 C16 H16 126.6 . . ?
C17 C16 H16 126.6 . . ?
O1 C17 C16 105.1(4) . . ?
O1 C17 H17A 110.7 . . ?
C16 C17 H17A 110.7 . . ?
O1 C17 H17B 110.7 . . ?
C16 C17 H17B 110.7 . . ?
H17A C17 H17B 108.8 . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.066
#===end

data_mf130
_database_code_depnum_ccdc_archive 'CCDC 848405'
#TrackingRef '2011_fustier_chemcommun.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H40 Fe2 P4 S4, 2 (C4 H8 O)'
_chemical_formula_sum            'C58 H56 Fe2 O2 P4 S4'
_chemical_formula_weight         1148.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'P-421c '
_symmetry_space_group_name_Hall  'P -4 2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   16.980(1)
_cell_length_b                   16.980(1)
_cell_length_c                   19.740(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5691.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    4518
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      30.034

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2384
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8549
_exptl_absorpt_correction_T_max  0.9840
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35123
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6506
_reflns_number_gt                5826
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_reduction        'DENZO & COLLECT'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Crystal was found to be twinned ; twin fraction 0.55/0.45
No centrosymmetric space group could be found to explain
flack parameter equal to 0.55 (0.02)
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.004 -0.003 0.500 727 189 ' '
2 -0.080 0.500 1.000 727 189 ' '
_platon_squeeze_details          
;
A highly disordered C4H8O molecule was accounted for using the
Platon SQUEEZE function.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+4.5870P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.55(3)
_refine_ls_number_reflns         6506
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1184
_refine_ls_wR_factor_gt          0.1144
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.5000 0.36358(3) 0.02821(15) Uani 1 2 d S . .
Fe2 Fe 0.5000 0.5000 0.23347(3) 0.02875(15) Uani 1 2 d S . .
S1 S 0.37601(6) 0.53872(6) 0.40890(6) 0.0416(2) Uani 1 1 d . . .
S2 S 0.53386(6) 0.37935(6) 0.18241(6) 0.0445(3) Uani 1 1 d . . .
P1 P 0.34387(5) 0.45637(5) 0.33981(5) 0.02928(19) Uani 1 1 d . . .
P2 P 0.45298(5) 0.34741(5) 0.25354(5) 0.03012(19) Uani 1 1 d . . .
C1 C 0.43041(19) 0.43221(18) 0.2979(2) 0.0271(6) Uani 1 1 d . . .
C2 C 0.2966(2) 0.3741(2) 0.38234(18) 0.0314(7) Uani 1 1 d . . .
C3 C 0.3249(2) 0.3494(3) 0.4447(2) 0.0439(9) Uani 1 1 d . . .
H3 H 0.3652 0.3784 0.4668 0.053 Uiso 1 1 calc R . .
C4 C 0.2945(3) 0.2825(3) 0.4745(2) 0.0572(12) Uani 1 1 d . . .
H4 H 0.3142 0.2652 0.5170 0.069 Uiso 1 1 calc R . .
C5 C 0.2346(3) 0.2399(3) 0.4421(3) 0.0567(13) Uani 1 1 d . . .
H5 H 0.2137 0.1938 0.4627 0.068 Uiso 1 1 calc R . .
C6 C 0.2059(3) 0.2645(3) 0.3805(3) 0.0524(11) Uani 1 1 d . . .
H6 H 0.1650 0.2359 0.3587 0.063 Uiso 1 1 calc R . .
C7 C 0.2371(2) 0.3312(2) 0.3505(2) 0.0401(9) Uani 1 1 d . . .
H7 H 0.2178 0.3480 0.3078 0.048 Uiso 1 1 calc R . .
C8 C 0.2660(2) 0.4954(2) 0.2853(2) 0.0364(8) Uani 1 1 d . . .
C9 C 0.1924(2) 0.5124(2) 0.3125(3) 0.0461(10) Uani 1 1 d . . .
H9 H 0.1831 0.5049 0.3596 0.055 Uiso 1 1 calc R . .
C10 C 0.1321(2) 0.5404(2) 0.2708(3) 0.0584(14) Uani 1 1 d . . .
H10 H 0.0816 0.5516 0.2892 0.070 Uiso 1 1 calc R . .
C11 C 0.1464(3) 0.5515(2) 0.2034(3) 0.0571(13) Uani 1 1 d . . .
H11 H 0.1053 0.5697 0.1748 0.068 Uiso 1 1 calc R . .
C12 C 0.2184(3) 0.5368(3) 0.1770(3) 0.0589(13) Uani 1 1 d . . .
H12 H 0.2278 0.5466 0.1303 0.071 Uiso 1 1 calc R . .
C13 C 0.2791(2) 0.5076(2) 0.2175(2) 0.0430(9) Uani 1 1 d . . .
H13 H 0.3291 0.4962 0.1982 0.052 Uiso 1 1 calc R . .
C14 C 0.3682(2) 0.3032(2) 0.21222(19) 0.0332(8) Uani 1 1 d . . .
C15 C 0.3285(2) 0.2403(2) 0.2412(2) 0.0386(9) Uani 1 1 d . . .
H15 H 0.3482 0.2166 0.2813 0.046 Uiso 1 1 calc R . .
C16 C 0.2598(2) 0.2120(2) 0.2115(2) 0.0454(10) Uani 1 1 d . . .
H16 H 0.2331 0.1685 0.2312 0.054 Uiso 1 1 calc R . .
C17 C 0.2302(3) 0.2466(2) 0.1539(3) 0.0497(11) Uani 1 1 d . . .
H17 H 0.1830 0.2273 0.1343 0.060 Uiso 1 1 calc R . .
C18 C 0.2689(3) 0.3088(3) 0.1247(2) 0.0519(11) Uani 1 1 d . . .
H18 H 0.2478 0.3332 0.0854 0.062 Uiso 1 1 calc R . .
C19 C 0.3390(3) 0.3364(2) 0.1527(2) 0.0452(10) Uani 1 1 d . . .
H19 H 0.3670 0.3779 0.1312 0.054 Uiso 1 1 calc R . .
C20 C 0.4947(2) 0.2690(2) 0.3043(2) 0.0372(8) Uani 1 1 d . . .
C21 C 0.4962(2) 0.2736(2) 0.3733(2) 0.0480(10) Uani 1 1 d . . .
H21 H 0.4763 0.3194 0.3950 0.058 Uiso 1 1 calc R . .
C22 C 0.5268(3) 0.2115(3) 0.4134(3) 0.0643(14) Uani 1 1 d . . .
H22 H 0.5268 0.2149 0.4615 0.077 Uiso 1 1 calc R . .
C23 C 0.5566(3) 0.1458(3) 0.3809(4) 0.082(2) Uani 1 1 d . . .
H23 H 0.5767 0.1030 0.4066 0.098 Uiso 1 1 calc R . .
C24 C 0.5571(3) 0.1424(3) 0.3097(5) 0.082(2) Uani 1 1 d . . .
H24 H 0.5793 0.0980 0.2875 0.098 Uiso 1 1 calc R . .
C25 C 0.5256(2) 0.2028(2) 0.2718(3) 0.0578(13) Uani 1 1 d . . .
H25 H 0.5250 0.1995 0.2237 0.069 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0281(3) 0.0245(3) 0.0321(3) 0.000 0.000 -0.0048(3)
Fe2 0.0284(3) 0.0250(3) 0.0328(3) 0.000 0.000 -0.0014(3)
S1 0.0345(4) 0.0385(5) 0.0518(6) -0.0211(4) 0.0060(4) -0.0040(4)
S2 0.0415(5) 0.0356(5) 0.0563(6) -0.0124(4) 0.0187(5) -0.0043(4)
P1 0.0257(4) 0.0245(4) 0.0376(5) -0.0057(4) 0.0022(4) -0.0015(3)
P2 0.0279(4) 0.0211(4) 0.0414(5) -0.0048(4) 0.0018(4) 0.0002(3)
C1 0.0284(16) 0.0225(15) 0.0304(15) -0.0021(13) 0.0011(13) -0.0012(10)
C2 0.0318(17) 0.0288(16) 0.0337(19) -0.0053(14) 0.0035(14) -0.0011(14)
C3 0.039(2) 0.053(2) 0.039(2) -0.0001(19) 0.0036(17) -0.0071(18)
C4 0.059(3) 0.068(3) 0.045(2) 0.014(2) 0.007(2) -0.008(2)
C5 0.058(3) 0.048(2) 0.064(3) 0.012(2) 0.016(2) -0.016(2)
C6 0.048(2) 0.048(3) 0.061(3) 0.000(2) 0.003(2) -0.018(2)
C7 0.0372(19) 0.0351(19) 0.048(2) -0.0018(17) -0.0020(17) -0.0079(15)
C8 0.0304(18) 0.0242(16) 0.055(2) -0.0056(17) -0.0058(15) 0.0048(14)
C9 0.0338(19) 0.0329(19) 0.072(3) -0.0030(19) 0.0016(19) 0.0031(15)
C10 0.0295(19) 0.033(2) 0.112(4) -0.008(2) -0.014(2) 0.0052(17)
C11 0.047(2) 0.035(2) 0.089(4) -0.006(2) -0.026(2) 0.0030(19)
C12 0.055(3) 0.047(2) 0.075(3) -0.006(2) -0.032(2) 0.006(2)
C13 0.041(2) 0.038(2) 0.051(2) -0.0030(19) -0.0100(17) 0.0023(17)
C14 0.0313(18) 0.0269(16) 0.041(2) -0.0117(14) 0.0000(15) 0.0007(14)
C15 0.0372(19) 0.0263(17) 0.052(2) -0.0034(16) -0.0086(17) -0.0007(14)
C16 0.034(2) 0.0273(18) 0.075(3) -0.0071(19) -0.0030(19) -0.0045(15)
C17 0.044(2) 0.042(2) 0.063(3) -0.022(2) -0.015(2) 0.0022(18)
C18 0.054(3) 0.053(3) 0.049(3) -0.003(2) -0.014(2) -0.003(2)
C19 0.050(2) 0.038(2) 0.047(2) -0.0055(18) 0.000(2) -0.0040(18)
C20 0.0274(17) 0.0255(17) 0.059(2) 0.0007(15) -0.0049(18) 0.0000(14)
C21 0.035(2) 0.0326(19) 0.076(3) 0.0099(19) 0.003(2) -0.0001(17)
C22 0.045(3) 0.058(3) 0.090(4) 0.034(3) -0.010(2) -0.003(2)
C23 0.047(3) 0.041(3) 0.156(7) 0.034(3) -0.018(3) 0.001(2)
C24 0.051(3) 0.029(2) 0.165(7) -0.009(3) -0.028(4) 0.011(2)
C25 0.041(2) 0.033(2) 0.100(4) -0.008(2) -0.013(2) 0.0091(16)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 2.099(3) 3_665 ?
Fe1 C1 2.099(3) . ?
Fe1 S1 2.3802(10) . ?
Fe1 S1 2.3802(10) 3_665 ?
Fe1 Fe2 2.5683(8) . ?
Fe1 P1 2.7923(9) 3_665 ?
Fe1 P1 2.7923(9) . ?
Fe2 C1 2.082(3) 3_665 ?
Fe2 C1 2.082(3) . ?
Fe2 S2 2.3545(10) . ?
Fe2 S2 2.3545(10) 3_665 ?
Fe2 P2 2.7400(8) . ?
Fe2 P2 2.7400(8) 3_665 ?
S1 P1 2.0281(13) . ?
S2 P2 2.0375(14) . ?
P1 C1 1.736(4) . ?
P1 C2 1.816(4) . ?
P1 C8 1.829(4) . ?
P2 C1 1.728(3) . ?
P2 C20 1.811(4) . ?
P2 C14 1.817(4) . ?
C2 C3 1.387(5) . ?
C2 C7 1.395(5) . ?
C3 C4 1.379(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.404(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.374(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.373(6) . ?
C8 C9 1.391(5) . ?
C9 C10 1.398(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.366(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.352(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.394(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.385(5) . ?
C14 C19 1.394(6) . ?
C15 C16 1.390(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.370(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.394(6) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.366(6) . ?
C20 C25 1.396(6) . ?
C21 C22 1.416(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.384(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.407(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.378(7) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C1 103.6(2) 3_665 . ?
C1 Fe1 S1 125.37(10) 3_665 . ?
C1 Fe1 S1 83.44(10) . . ?
C1 Fe1 S1 83.45(10) 3_665 3_665 ?
C1 Fe1 S1 125.37(10) . 3_665 ?
S1 Fe1 S1 135.85(6) . 3_665 ?
C1 Fe1 Fe2 51.82(10) 3_665 . ?
C1 Fe1 Fe2 51.82(10) . . ?
S1 Fe1 Fe2 112.08(3) . . ?
S1 Fe1 Fe2 112.08(3) 3_665 . ?
C1 Fe1 P1 38.38(10) 3_665 3_665 ?
C1 Fe1 P1 125.18(10) . 3_665 ?
S1 Fe1 P1 146.06(3) . 3_665 ?
S1 Fe1 P1 45.30(3) 3_665 3_665 ?
Fe2 Fe1 P1 80.33(2) . 3_665 ?
C1 Fe1 P1 125.18(10) 3_665 . ?
C1 Fe1 P1 38.38(10) . . ?
S1 Fe1 P1 45.30(3) . . ?
S1 Fe1 P1 146.06(3) 3_665 . ?
Fe2 Fe1 P1 80.33(2) . . ?
P1 Fe1 P1 160.65(5) 3_665 . ?
C1 Fe2 C1 104.78(19) 3_665 . ?
C1 Fe2 S2 127.13(10) 3_665 . ?
C1 Fe2 S2 85.35(10) . . ?
C1 Fe2 S2 85.34(10) 3_665 3_665 ?
C1 Fe2 S2 127.13(10) . 3_665 ?
S2 Fe2 S2 129.31(6) . 3_665 ?
C1 Fe2 Fe1 52.39(10) 3_665 . ?
C1 Fe2 Fe1 52.39(10) . . ?
S2 Fe2 Fe1 115.35(3) . . ?
S2 Fe2 Fe1 115.35(3) 3_665 . ?
C1 Fe2 P2 126.86(10) 3_665 . ?
C1 Fe2 P2 39.08(9) . . ?
S2 Fe2 P2 46.39(3) . . ?
S2 Fe2 P2 144.44(3) 3_665 . ?
Fe1 Fe2 P2 81.69(2) . . ?
C1 Fe2 P2 39.08(9) 3_665 3_665 ?
C1 Fe2 P2 126.86(10) . 3_665 ?
S2 Fe2 P2 144.45(3) . 3_665 ?
S2 Fe2 P2 46.39(3) 3_665 3_665 ?
Fe1 Fe2 P2 81.69(2) . 3_665 ?
P2 Fe2 P2 163.38(5) . 3_665 ?
P1 S1 Fe1 78.16(4) . . ?
P2 S2 Fe2 76.82(4) . . ?
C1 P1 C2 114.39(16) . . ?
C1 P1 C8 114.62(18) . . ?
C2 P1 C8 103.35(17) . . ?
C1 P1 S1 104.83(11) . . ?
C2 P1 S1 109.76(12) . . ?
C8 P1 S1 109.93(13) . . ?
C1 P1 Fe1 48.64(11) . . ?
C2 P1 Fe1 123.08(12) . . ?
C8 P1 Fe1 133.57(13) . . ?
S1 P1 Fe1 56.54(3) . . ?
C1 P2 C20 114.83(18) . . ?
C1 P2 C14 113.32(16) . . ?
C20 P2 C14 104.72(17) . . ?
C1 P2 S2 106.06(12) . . ?
C20 P2 S2 108.26(14) . . ?
C14 P2 S2 109.56(13) . . ?
C1 P2 Fe2 49.44(11) . . ?
C20 P2 Fe2 131.43(12) . . ?
C14 P2 Fe2 123.83(12) . . ?
S2 P2 Fe2 56.79(4) . . ?
P2 C1 P1 128.78(17) . . ?
P2 C1 Fe2 91.48(16) . . ?
P1 C1 Fe2 129.86(18) . . ?
P2 C1 Fe1 130.18(19) . . ?
P1 C1 Fe1 92.98(16) . . ?
Fe2 C1 Fe1 75.79(10) . . ?
C3 C2 C7 119.5(4) . . ?
C3 C2 P1 119.4(3) . . ?
C7 C2 P1 120.9(3) . . ?
C4 C3 C2 119.9(4) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 120.1(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 C4 120.2(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 119.4(4) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C6 C7 C2 120.9(4) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
C13 C8 C9 119.4(4) . . ?
C13 C8 P1 120.8(3) . . ?
C9 C8 P1 119.8(3) . . ?
C8 C9 C10 120.1(5) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 119.4(4) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C12 C11 C10 120.7(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 120.9(5) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C8 C13 C12 119.5(4) . . ?
C8 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C15 C14 C19 119.1(4) . . ?
C15 C14 P2 121.3(3) . . ?
C19 C14 P2 119.5(3) . . ?
C14 C15 C16 120.1(4) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C17 C16 C15 120.5(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 120.1(4) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 120.1(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C14 C19 C18 120.1(4) . . ?
C14 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C25 119.8(4) . . ?
C21 C20 P2 121.2(3) . . ?
C25 C20 P2 119.0(3) . . ?
C20 C21 C22 121.5(4) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C23 C22 C21 118.3(6) . . ?
c23 C22 H22 120.8 . . ?
C21 C22 H22 120.8 . . ?
C22 C23 C24 120.0(5) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 120.6(5) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C20 119.7(6) . . ?
C24 C25 H25 120.1 . . ?
C20 C25 H25 120.1 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.060
#===end